HRID426272

反应详情

EQUATION

反应方程式

HRID 426272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-2,6-dimethoxy-pyrimidine (2.2 g, 12.6 mmol) and sodium bicarbonate (2.39 g, 28.4 mmol) were stirred in aqueous methanol (50%, 40 mL) at room temperature. Bromine (3.52 g, 22.0 mmol) was added dropwise over a period of 60 minutes. After the addition was complete, stirring was continued or additional 60 minutes. The solid was collected and was washed with water to yield 6.2 g of crude material. 3.1 g of the crude material were dissolved in hot methanol (40 mL) and water (10 mL) was added. The resultant precipitate was collected and dried in vacuo to yield the product (1.0 g, 3.95 mmol). 1H (CDCl3): δ=4.05 (s, 3H), 3.99 (s, 3H) ppm.

WORKUP

后处理

  1. additionAfter the addition
  2. customThe solid was collected
  3. washwas washed with water
  4. customto yield 6.2 g of crude material
  5. customThe resultant precipitate was collected
  6. customdried in vacuo